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Scanning Probe Investigations of Multidentate Thiol and Spatially Confined Porphyrin Nanoassemblies Using Nanoscale Lithography" (2016)

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Scanning Probe Investigations of Multidentate Thiol and Spatially Confined Porphyrin Nanoassemblies Using Nanoscale Lithography Louisiana State University LSU Digital Commons LSU Doctoral Dissertations Graduate School 2016 Scanning Probe Investigations of Multidentate Thiol nda Spatially Confined orP phyrin Nanoassemblies using Nanoscale Lithography Xianglin Zhai Zhai Louisiana State University and Agricultural and Mechanical College, [email protected] Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_dissertations Part of the Chemistry Commons Recommended Citation Zhai, Xianglin Zhai, "Scanning Probe Investigations of Multidentate Thiol and Spatially Confined Porphyrin Nanoassemblies using Nanoscale Lithography" (2016). LSU Doctoral Dissertations. 2050. https://digitalcommons.lsu.edu/gradschool_dissertations/2050 This Dissertation is brought to you for free and open access by the Graduate School at LSU Digital Commons. It has been accepted for inclusion in LSU Doctoral Dissertations by an authorized graduate school editor of LSU Digital Commons. For more information, please [email protected]. SCANNING PROBE INVESTIGATIONS OF MULTIDENTATE THIOL AND SPATIALLY CONFINED PORPHYRIN NANOASSEMBLIES USING NANOSCALE LITHOGRAPHY A Dissertation Submitted to the Graduate Faculty of the Louisiana State University and Agricultural and Mechanical College in partial fulfillment of the requirements for the degree of Doctor of Philosophy in The Department of Chemistry by Xianglin Zhai B.S., Northeast Forestry University, 2006 M.S., Northeast Forestry University, 2009 May 2016 ACKNOWLEDGMENTS I would like to thank my advisor, Dr. Jayne C. Garno. She has truly given me the encouragement, inspiration, and guidance needed during my time at LSU. I would like to thank her for affording me the opportunity to work in her group, and for playing an instrumental role in my academic success. She is truly a woman who cares about the success of her students. I would also like to thank Dr. Justin Ragains, my collaborator. He has been a blessing as both a mentor and a role model during my graduate career. Thank you to my committee members Dr. Bin Chen, Dr. Louis Haber, and Dr. Kevin S. McCarter for reviewing my dissertation and providing valuable feedback. To the Garno group (both past and present), the blood, sweat, and tears we shared will always be held close to my heart. It was truly a pleasure to work for a group with such a nurturing and collaborative spirit. I will miss all of the tailgates, lunches, group parties, and conference trips we’ve shared over the years. I hope to stay in touch with each of you, and wish you all the success in the future. Specifically, I like to acknowledge my colleagues, Dr. Tian Tian, Dr. Lauren Englade-Franklin, Dr. ChaMarra Saner, and Dr. Susan Sutton. Each of you has played an integral role in my research in some way, and for that I will be forever grateful. More importantly, you have each become a friend, and I cannot express how much this means to me personally. To my parents Xilan Zhai and Guilan Yue, I must say thank you for always putting up with me! Your love and support have led me to where I am today. Mom, you are the strongest woman I have ever met. Thank you for always standing up for what is right, and being the amazing role model you are. You’ve always been there for me, and I can’t tell you how much I love you. Dad, you have pushed me to always succeed and never give up. Thank you for teaching me what is ii worth fighting and working for in life, I love you. I would also like to thank my families in China. Your love is the powerful and secure backing for me whenever I was facing difficulties in my life. Finally, I would like to express my gratitude and love to my darlings, Zheng Xue and Sophia S. Zhai. It is a huge bless that I have you in my life. Thank you my wife, Zheng Xue for always believing in me when I doubt myself. I would not step so far without your support. Thank you my beloved Sophia, thank you for being in my life. Your arrival to my life made me grown, tough and fearless to my unknown future. You are both my families, my love and my best friends. I love you both forever! iii TABLE OF CONTENTS ACKNOWLEDGMENTS .............................................................................................................. ii LIST OF TABLE .......................................................................................................................... vii LIST OF SCHEMES.................................................................................................................... viii LIST OF FIGURES ....................................................................................................................... ix LIST OF ABBREVIATIONS ...................................................................................................... xiv ABSTRACT ...................................................................................................................................xv CHAPTER 1: INTRODUCTION ....................................................................................................1 1.1 Nanoscale studies using scanning probe microscopy (SPM) ................................................ 1 1.2 Self-assembly of bidentate thiol on Au(111) studied with AFM3 ......................................... 1 1.3 Measurement of spatially confined nanoclusters of porphyrins using CP-AFM .................. 2 1.4 Nanorods derived from porphyrins characterized with CP-AFM ......................................... 3 1.5 Synopsis ................................................................................................................................ 4 CHAPTER 2: ATOMIC FORCE MICROSCOPY .........................................................................5 2.1 Overview of scanning probe microscopy .............................................................................. 5 2.2 Imaging modes of AFM ........................................................................................................ 8 2.2.1 Contact mode AFM and lateral force imaging ............................................................... 8 2.2.2 Tapping mode AFM and phase imaging ...................................................................... 11 2.3 Force-distance curve ........................................................................................................... 12 2.4 Liquid imaging .................................................................................................................... 14 2.5 Scanning probe fabrication.................................................................................................. 15 2.5.1 Nanoshaving ................................................................................................................. 16 2.5.2 Nanografting ................................................................................................................. 18 2.6 Conductive-probe AFM ...................................................................................................... 20 2.7 Self-assembled monolayers of organosulfur ....................................................................... 23 2.8 Particle lithography ............................................................................................................. 24 CHAPTER 3: NANOSCALE LITHOGRAPHY MEDIATED BY SURFACE SELF- ASSEMBLY OF 16-[3,5-BIS(MERCAPTOMETHYL)PHENOXY]HEXADECANOIC ACID ON AU(111) INVESTIGATED WITH SCANNING PROBE MICROSCOPY3* .......................26 3.1 Introduction ......................................................................................................................... 26 3.2 Materials and methods ........................................................................................................ 29 3.2.1 Materials ....................................................................................................................... 29 3.2.2 Preparation of organic thin films on Au(111) .............................................................. 29 3.2.3 Preparation of template-stripped Au(111) .................................................................... 29 3.2.4 Immersion particle lithography with masks of silica mesoparticles ............................. 30 3.2.5 Atomic force microscopy ............................................................................................. 30 3.2.6 Scanning probe-based nanolithography (nanoshaving and nanografting) ................... 31 3.3 Results and discussion ......................................................................................................... 32 iv 3.3.1 Nanoshaving within a monolayer film of BMPHA ...................................................... 33 3.3.2 Nanografting n-alkanethiols within a monolayer of BMPHA...................................... 34 3.3.3 Nanografting ODT within a double layer of BMPHA ................................................. 38 3.3.4 Nanofabrication experiments with BMPHA using immersion particle lithography .... 40 3.4 Conclusions ......................................................................................................................... 45 CHAPTER 4: CONDUCTIVE-PROBE MEASUREMENTS WITH NANODOTS OF FREE- BASE AND METALLATED PORPHYRINS ..............................................................................46 4.1 Introduction ......................................................................................................................... 46 4.2 Materials and methods .......................................................................................................
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